Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof

An organometallic and catalyst technology, applied in the field of nano-spherical mesoporous organometallic catalysts, to achieve the effect of preventing pollution and simple operation

Inactive Publication Date: 2010-07-14
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no report on the preparation of mesoporous organometallic catalysts by spray drying

Method used

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  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof
  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof
  • Nano-spherical mesoporous organic metal catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of catalyst: At room temperature, a mixture of 1.6g of surfactant CTAB (0.0044mol), 33ml of ethanol (0.57mol), 0.39g of sodium chloride, 6.5ml of water and 0.22ml of aqueous hydrochloric acid (2M) was stirred for 1 After ~6 hours, add 4.3 ml of inorganic silicon source TEOS (0.019 mol), pre-hydrolyze for 1 hour, add 0.27 g (0.00029 mol) of freshly prepared bis-(1-triethoxysilicon-2 dissolved in 2 ml of tetrahydrofuran) -diphenylphosphine)ethane palladium dichloride (organometallic palladium silicon source), continue stirring for 1 to 3 hours until it becomes a homogeneous solution. Subsequently, after spray drying at 573K and 1Mpa pressure, extraction and washing with ethanol at 353K for 24 hours, and vacuum drying, a milky yellow solid powder was obtained, which was a nano-spherical ordered mesoporous organometallic catalyst with high specific surface area. Pd(II)- MOC-AASA said. The content of Pd in ​​the product is 0.14 mmol / g (2% by mass), and the activ...

Embodiment 2

[0032]Take 0.014ml iodobenzene (0.125mmol), 0.014ml phenylacetylene (0.125mmol), 0.030ml n-heptane (internal standard), 0.21ml DBU (1,8-diazacyclo[5,4,0]ten Monoene-7) (1.48mmol), 0.0050g cocatalyst cuprous iodide (0.0259mmol), 4.0ml deionized water, Pd(II)-MOC-AASA prepared in Example 1 (Pd content is 0.005mmol) , and reacted at 353K for 5h. After the obtained product was extracted 5 times with 10ml of toluene, the reaction product was analyzed by gas chromatograph (Agilent GC1790). The analysis results are shown in Table 1.

[0033] Catalytic performance of catalysts in Table 1 Examples 1 and 2

[0034]

Embodiment 3

[0036] Carry out the activity test of benzaldehyde homologues according to the Barbier reaction system of Example 1, take equimolar number of different para-substituents of benzaldehyde as reaction substrates, and reaction conditions and detection means are the same as in Example 1. The analysis results are shown in Table 2.

[0037] The catalytic performance of the catalyst in Table 2 Example 3

[0038]

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Abstract

The invention discloses a nano-spherical mesoporous organic metal catalyst. In the nano-spherical mesoporous organic metal catalyst, the grain diameter is between 100 and 600nm, the pore diameter is between 1.5 and 8.0nm, the pore volume is between 0.2 and 1.0cm<3> / g, the specific surface area is between 800 and 1,200m<2> / g, and the Pd element content is between 0.05 and 0.35mmol / g. The preparation method comprises the following steps: mixing organic metal silane, solution of inorganic silane, a template, water and ethanol; performing a hydrolytic polycondensation reaction by using a spray drying method; and extracting the template from an obtained solid by using alcohols to prepare the nano-spherical mesoporous organic metal catalyst. By using the method, an organic metallic catalyst with ordered mesopore arrangement can be quickly prepared, the active ingredients of the organic metallic catalyst are highly dispersed in pore passages, and the organic metallic catalyst serves as a catalyst for Barbier reaction or Sonogashira reaction in a water medium, and the organic metallic catalyst can have the catalytic performance similar to that of a homogenous organic metal catalyst.

Description

technical field [0001] The invention relates to a nano-spherical mesoporous organometallic catalyst, in particular to its preparation scheme and the application of the catalytic material in cleaning organic reactions in an aqueous medium. Background technique [0002] Water is the most harmless substance and the safest solvent on earth. As a green non-polluting reaction medium, it has always been widely concerned by people. In recent years, the use of water instead of organic solvents for organic synthesis reactions has become an important branch of green chemistry. At present, homogeneous organometallic catalysts are mostly used in aqueous media due to their high activity and selectivity. However, due to their difficulty in separating and recycling from the reaction system, it is difficult to make breakthroughs in industrial applications. In addition, homogeneous catalysts It will also bring heavy metal ion pollution. In order to solve the above problems, people generally...

Claims

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Application Information

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IPC IPC(8): B01J31/12B01J35/10B01J37/08C07C33/30C07C29/38C07C15/54C07C2/86
Inventor 张昉康春梅李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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